DE3634492C2 - Method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic - Google Patents

Method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic

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Publication number
DE3634492C2
DE3634492C2 DE19863634492 DE3634492A DE3634492C2 DE 3634492 C2 DE3634492 C2 DE 3634492C2 DE 19863634492 DE19863634492 DE 19863634492 DE 3634492 A DE3634492 A DE 3634492A DE 3634492 C2 DE3634492 C2 DE 3634492C2
Authority
DE
Germany
Prior art keywords
metal
body made
tight
sintered
layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
DE19863634492
Other languages
German (de)
Other versions
DE3634492A1 (en
Inventor
Klaus Prof Dr Bente
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Endress and Hauser Deutschland Holding GmbH
Original Assignee
Fischer and Porter GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fischer and Porter GmbH filed Critical Fischer and Porter GmbH
Priority to DE19863634492 priority Critical patent/DE3634492C2/en
Priority to GB8723321A priority patent/GB2196568B/en
Publication of DE3634492A1 publication Critical patent/DE3634492A1/en
Application granted granted Critical
Publication of DE3634492C2 publication Critical patent/DE3634492C2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F1/00—Measuring the volume flow or mass flow of fluid or fluent solid material wherein the fluid passes through a meter in a continuous flow
    • G01F1/56—Measuring the volume flow or mass flow of fluid or fluent solid material wherein the fluid passes through a meter in a continuous flow by using electric or magnetic effects
    • G01F1/58—Measuring the volume flow or mass flow of fluid or fluent solid material wherein the fluid passes through a meter in a continuous flow by using electric or magnetic effects by electromagnetic flowmeters
    • G01F1/584—Measuring the volume flow or mass flow of fluid or fluent solid material wherein the fluid passes through a meter in a continuous flow by using electric or magnetic effects by electromagnetic flowmeters constructions of electrodes, accessories therefor
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
    • C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12—Metallic interlayers
    • C04B2237/122—Metallic interlayers based on refractory metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12—Metallic interlayers
    • C04B2237/123—Metallic interlayers based on iron group metals, e.g. steel
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12—Metallic interlayers
    • C04B2237/125—Metallic interlayers based on noble metals, e.g. silver
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/34—Oxidic
    • C04B2237/343—Alumina or aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C04B2237/403—Refractory metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/60—Forming at the joining interface or in the joining layer specific reaction phases or zones, e.g. diffusion of reactive species from the interlayer to the substrate or from a substrate to the joining interface, carbide forming at the joining interface
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/70—Forming laminates or joined articles comprising layers of a specific, unusual thickness
    • C04B2237/708—Forming laminates or joined articles comprising layers of a specific, unusual thickness of one or more of the interlayers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
    • C04B2237/765—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc at least one member being a tube

Description

Die Erfindung betrifft ein Verfahren zum Herstellen einer vakuumdichten und druckdichten Verbindung zwischen einem Körper aus Metall und einem Körper aus gesinterter Oxidkeramik, in den der Körper aus Metall eingesintert ist.The invention relates to a method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic, in which the body is sintered in metal.

Aus der US-PS 3 706 582 ist es bekannt, eine feste und dichte Verbindung zwischen Keramik und Platin über die Ausbildung silikatischer Phasen herbeizuführen.From US-PS 3 706 582 it is known to be solid and tight Connection between ceramic and platinum through training bring about silicate phases.

Aus der DE-PS 33 18 585 ist ein Verfahren zur Herstellung einer vakuumdichten Verbindung zwischen einer Oxidkeramik und einem keramischen Leiter aus Platin oder eine Platinlegierung be­ kannt, bei dem der Leiter vor dem Sintern der Oxidkeramik in eine Bohrung der Oxidkeramik eingesetzt oder durch Spritzpres­ sen oder durch Spritzgießen mit der oxidkeramischen Masse umspritzt wird, so daß er von der Oxidkeramik in allseitigem unmittelbarem Kontakt umgeben ist, wonach ein Sintern mit einer Sintertemperatur erfolgt, die unterhalb der Schmelztemperatur des elektrischen Leiters liegt und beim Sintern Kristallite in die Oberfläche des Leiters hineinwachsen.From DE-PS 33 18 585 is a method for producing a vacuum-tight connection between an oxide ceramic and a ceramic conductor made of platinum or a platinum alloy knows, in which the conductor before sintering the oxide ceramic in a hole in the oxide ceramic used or by injection molding sen or by injection molding with the oxide ceramic mass is overmolded so that it is coated on all sides by the oxide ceramic immediate contact, after which sintering with a Sintering temperature takes place below the melting temperature of the electrical conductor and crystallites during sintering grow the surface of the conductor into it.

Aus der EP 0 080 535 A1 ist ein Verfahren zur Befestigung von Meßelektroden und anderer stromleitender Bauteile an einem keramischen Meßrohr eines Meßwertaufnehmers für magnetisch­ induktive Durchflußmeßgeräte bekannt, bei dem Schäfte der Meßelektroden in einer radial durch den Mantel des Meßrohrs führenden Lage befestigt werden, wobei der Schaft jeder Meß­ elektrode in einem aus Oxidkeramik-Rohstoff bestehenden unge­ brannten Formling radial angeordnet und beim keramischen Bren­ nen des Formlings eingesintert wird. Als Meßelektroden und Schäfte können Platin oder Platinlegierungen verwendet werden. Das Meßrohr kann aus dicht gesintertem Aluminiumoxid bestehen und die Schäfte bei etwa 1800°C eingesintert werden. Der unge­ brannte Formling des Meßrohrs kann in einer Stempelpresse oder isostatisch gepreßt werden, und anschließend können in ihm radiale Bohrungen zum Einstecken der Schäfte vorgesehen werden.EP 0 080 535 A1 describes a method for fastening Measuring electrodes and other current-carrying components on one Ceramic measuring tube of a sensor for magnetic known inductive flow meters, in which the shafts Measuring electrodes in a radial through the jacket of the measuring tube leading position are attached, the shaft of each measuring electrode in a container made of oxide ceramic raw material fired blank arranged radially and in ceramic firing sintered of the molding. As measuring electrodes and Shafts can be made of platinum or platinum alloys. The measuring tube can consist of densely sintered aluminum oxide and the shafts are sintered in at about 1800 ° C. The boy Burnt blank of the measuring tube can be in a stamp press or can be pressed isostatically, and then in it radial bores are provided for inserting the shafts.

Aufgabe der Erfindung ist es, ein Verfahren nach dem Oberbe­ griff des Anspruchs 1 anzugeben, das mit äußerst geringer Ausschußquote, wenn überhaupt einer Ausschußquote, eine siche­ re, vakuumdichte und druckdichte Verbindung erreichen läßt.The object of the invention is a method according to the Oberbe handle of claim 1 specify that with extremely low Reject rate, if any, is a safe rate re, vacuum-tight and pressure-tight connection can be achieved.

Die Lösung dieser Aufgabe ist im Kennzeichen des Anspruchs 1 angegeben.The solution to this problem is in the characterizing part of claim 1 specified.

Durch das Verfahren wird eine unmittelbare Grenzfläche zwischen dem Körper aus Metall, also insbesondere dem Platindraht und der Schicht aus Aluminium bzw. anderer Metalle, geschaffen. Vor oder während des Sinterns werden die Metallschichten, vorzugs­ weise Aluminium, oxidiert und erfahren so ein Dickenwachstum, das dem gleichzeitigen Schrumpfungsvorgang des Körpers aus Oxidkeramik, also insbesondere aus der Al₂O₃-Keramik, im Sinne des stärkeren mechanischen Einklemmens des Körpers aus Metall, also insbesondere des Platindrahts, geometrisch gesehen ent­ gegenwirkt. Die starke mechanische Einklemmung des Körpers aus Metall, die hierdurch erreicht wird, wird noch erhöht durch das Zusammensintern der zu Al₂O₃ oder anderen auch höher polynären Oxiden gewordenen Grenzschicht und des Körpers aus Oxidkeramik.The process creates an immediate interface between the body made of metal, in particular the platinum wire and the layer of aluminum or other metals. In front or during sintering, the metal layers are preferred wise aluminum, oxidizes and experiences a growth in thickness, the simultaneous shrinking process of the body Oxide ceramics, in particular from Al₂O₃ ceramics, in the sense the stronger mechanical clamping of the metal body, in particular the platinum wire, seen geometrically counteracts. The strong mechanical pinching of the body Metal that is achieved in this way is further increased by the Sintering together to form Al₂O₃ or other polynaires Boundary layer that has become oxide and the body made of oxide ceramic.

Ein besonders inniger Übergang zwischen der Aluminiumschicht und dem Körper aus Metall ergibt sich, wenn das Aluminium im Hochvakuum aufgedampft wird. Hierbei sind folgende Bemessungen vorteilhaft:
Aufdampfung von hochreinem Aluminium (99,99%) bei einem Vakuum von besser als 10 exp. -8 bar. Galvanisch oder durch andere Methoden aufgebrachte Metalle sind ebenfalls in einer Reinheit von mindestens 99,9% zu verwenden.A particularly intimate transition between the aluminum layer and the metal body results when the aluminum is evaporated in a high vacuum. The following dimensions are advantageous:
Evaporation of high-purity aluminum (99.99%) with a vacuum of better than 10 exp. -8 bar. Metals applied galvanically or by other methods must also be used in a purity of at least 99.9%.

Claims (8)

1. Verfahren zum Herstellen einer vakuumdichten und druck­ dichten Verbindung zwischen einem Körper aus Metall und einem Körper aus gesintert Oxidkeramik, in den der Kör­ per aus Metall eingesintert wird, dadurch gekennzeichnet, daß wenigstens diejenigen Bereiche des Körpers aus Metall, die mit dem Körper aus Oxidkeramik verbunden werden, mit einer Metallschicht versehen werden und diese Metall­ schicht vor oder während des Sinterns oxidiert wird.1. A method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic, in which the body is sintered by metal, characterized in that at least those areas of the body made of metal which are made with the body Oxide ceramics are connected, provided with a metal layer and this metal layer is oxidized before or during sintering. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Oxidkeramik eine gesinterte Al₂O₃-Keramik verwendet wird.2. The method according to claim 1, characterized in that as Oxide ceramic a sintered Al₂O₃ ceramic is used. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß für den Körper aus Metall ein Platindraht verwendet wird, der als Elektrode in eine Wand eines aus der gesinterten Al₂O₃-Keramik beste­ henden Meßrohrs ein Durchflußmeß­ geräts eingesintert wird. 3. The method according to claim 2, characterized in that for the Body made of metal a platinum wire is used as the electrode in a wall of the best from the sintered Al₂O₃ ceramic measuring tube a flow meter device is sintered.   4. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß die Bereiche mit einer Metallschicht aus Al, Ni, Cr oder Fe versehen werden.4. The method according to any one of the preceding claims, characterized characterized in that the areas with a metal layer made of Al, Ni, Cr or Fe. 5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß eine Schicht aus Aluminium auf den Körper aus Metall im Hochvakuum aufgedampft wird.5. The method according to any one of the preceding claims, characterized characterized in that a layer of aluminum on the Metal body is evaporated in a high vacuum. 6. Verfahren nach einem der Ansprüche 1 bis 4, dadurch ge­ kennzeichnet, daß eine Schicht aus einem anderen Metall als Aluminium auf den Körper aus Metall galvanisch aufge­ bracht wird.6. The method according to any one of claims 1 to 4, characterized ge indicates that a layer of another metal galvanically applied to the metal body as aluminum is brought. 7. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß die Schicht aus Aluminium in einer Dicke bis 0,002 mm aufgebracht wird.7. The method according to claim 5, characterized in that the Layer of aluminum is applied in a thickness of up to 0.002 mm. 8. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die Schicht aus einem anderen Metall als Aluminium in einer Dicke bis zu 0,1 mm, vorzugsweise von 0,02 mm, aufgebracht wird.8. The method according to claim 6, characterized in that the Layer of a metal other than aluminum in a thickness up to 0.1 mm, preferably 0.02 mm, is applied.
DE19863634492 1986-10-09 1986-10-09 Method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic Expired - Fee Related DE3634492C2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE19863634492 DE3634492C2 (en) 1986-10-09 1986-10-09 Method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic
GB8723321A GB2196568B (en) 1986-10-09 1987-10-05 A metal-ceramic seal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19863634492 DE3634492C2 (en) 1986-10-09 1986-10-09 Method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic

Publications (2)

Publication Number Publication Date
DE3634492A1 DE3634492A1 (en) 1988-04-14
DE3634492C2 true DE3634492C2 (en) 1995-04-13

Family

ID=6311434

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19863634492 Expired - Fee Related DE3634492C2 (en) 1986-10-09 1986-10-09 Method for producing a vacuum-tight and pressure-tight connection between a body made of metal and a body made of sintered oxide ceramic

Country Status (2)

Country Link
DE (1) DE3634492C2 (en)
GB (1) GB2196568B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5273203A (en) * 1989-12-21 1993-12-28 General Electric Company Ceramic-to-conducting-lead hermetic seal
US5241216A (en) * 1989-12-21 1993-08-31 General Electric Company Ceramic-to-conducting-lead hermetic seal
US6521350B2 (en) * 2001-06-18 2003-02-18 Alfred E. Mann Foundation For Scientific Research Application and manufacturing method for a ceramic to metal seal

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3706582A (en) * 1968-09-20 1972-12-19 Gte Sylvania Inc Glass frit-ceramic powder composition
GB1409867A (en) * 1972-08-28 1975-10-15 Buckbee Mears Co Bonding of members to ceramic articles
ATE15270T1 (en) * 1981-11-27 1985-09-15 Rheometron Ag MEASURING TRANSDUCER FOR MAGNETIC-INDUCTION FLOWMETERING DEVICES.
US4500383A (en) * 1982-02-18 1985-02-19 Kabushiki Kaisha Meidensha Process for bonding copper or copper-chromium alloy to ceramics, and bonded articles of ceramics and copper or copper-chromium alloy
DE3318585A1 (en) * 1983-05-21 1984-11-22 Friedrichsfeld Gmbh, Steinzeug- Und Kunststoffwerke, 6800 Mannheim Process for making a vacuum-tight bond, and a composite produced thereby

Also Published As

Publication number Publication date
GB2196568B (en) 1991-03-27
DE3634492A1 (en) 1988-04-14
GB8723321D0 (en) 1987-11-11
GB2196568A (en) 1988-05-05

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Owner name: ENDRESS + HAUSER (DEUTSCHLAND) HOLDING GMBH, 79576

8339 Ceased/non-payment of the annual fee